CN102898651A - Preparation method of vinylphenyl silicon resin for LED (light-emitting diode) packaging - Google Patents
Preparation method of vinylphenyl silicon resin for LED (light-emitting diode) packaging Download PDFInfo
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Abstract
The invention relates to a preparation method of an organic silicon resin, particularly a preparation method of a vinylphenyl silicon resin for LED (light-emitting diode) packaging. The preparation method comprises the following steps: 1) adding water into a kettle, and adding a solvent; 2) adding a blocking agent, stirring, and adding an acidic catalyst; 3) stirring the mixed solution at normal temperature, dropwisely adding an ethanol solution of one or more of phenyl alkoxy silane, vinyl alkoxy silane and ethyl orthosilicate at 0-60 DEG C; 4) after finishing the dropwise addition, hydrolyzing for 30-600 minutes; 5) standing for 5-30 hours to stratify; and 6) treating with a condensation additive for an oil solution, and removing low boilers, thereby obtaining the product vinylphenyl silicon resin. The invention has the advantages of cheap and accessible raw materials, mild conditions and simple technique, and is simple to operate and convenient for industrialization.
Description
Technical field
The present invention relates to a kind of preparation method of silicone resin, specifically refer to the preparation method for the silicone resin of the ethenylphenyl of LED encapsulation.
Background technology
LED, incandescent light, luminescent lamp that contrast is used at present, a kind of more energy-conservation more environmental protection lighting system higher to technical requirements, its power consumption only is 1/10 of these conventional light source, do not use the mercury of serious environment pollution, volume is little, and the life-span is long, be expected to become after incandescent light, luminescent lamp, high-intensity gas discharge lamp the 4th generation light source.Can say, the LED development of high brightness is the breakthrough to the revolution of lighting engineering.
At present, the packaged material of common LED mainly is transparent epoxy resin, along with the development of white light LEDs, needs packaged material can higher specific absorption be arranged to UV-light when keeping the visible region high transparent, to prevent ultraviolet leakage; In addition, packaged material also needs to have stronger ultra-violet radiation resisting ability.Yellowing can occur in Resins, epoxy inevitably under the UV-irradiation of led chip emission behind life-time service, cause transmittance to descend, and the brightness of LED device reduces.The Resins, epoxy thermal resistance is very high in addition, because the bad meeting of dispelling the heat causes junction temperature of chip to rise rapidly, thereby accelerates the device light decay, even can be because the stress that rapid thermal expansion produces causes cracking.Therefore, along with the develop rapidly of LED research and development, also more and more higher to the requirement of packaged material, the power of LED is also increasing, and traditional epoxy resin encapsulating material can't satisfy high-power requirement gradually.And organosilicon have well heat-resisting, fast light, insulate, refuse the good characteristic such as water, also have very high transparency, with respect to general Resins, epoxy, have quite low thermal impedance, low approximately nearly 30%, as the LED packaged material, its performance is far superior to Resins, epoxy.The large power white light LED packaged material also requires to have certain hardness, tensile strength except requiring very high refractive index, transmittance and UV resistant radiation.Phenyl polysiloxane is as closed material, has that specific refractory power is high, light transmission good, good reinforcing effect is arranged, and has a extensive future.
Now, domestic had some units that this is studied.The patent No. CN101979427A of the yellow high honour of the scientific and technological Group Co.,Ltd of Yangzhou morningization etc. is by synthesis of vinyl phenyl polysiloxanes that is hydrolyzed such as phenyl chlorosilane, methyl chlorosilane, methyl ethylene chlorosilane and methyl closure agent, methyl ethylene closure agents; The patent No. CN101654560A of Maoming Xinyi Chemical Co., Ltd. and Ke Song, the phenyl polysiloxane of making by front three, phenyl-trichloro-silicane, vinyl-dimethyl base oxethyl silane, vinyltriethoxysilane, tetraethoxy; With the hydrogeneous resin of phenyl made from front three, methyl hydrogen dichlorosilane, hexichol dichlorosilane, aminomethyl phenyl diethoxy silane etc., make LED silicon rubber; The patent No. CN101343365A of the refined grade of the Wu Lian of Hangzhou Pedagogic University also is by synthesis of vinyl base phenyl polysiloxanes that is hydrolyzed such as phenyl trichlorine, aminomethyl phenyl dichloro, hexichol dichloro, methyl ethylene dichloro, methyl trichlorine, trimethylchlorosilanes; Hangzhou Pedagogic University comes the patent No. CN101475689B of state's bridge etc., adopts octadecyloxy phenyl TMOS, methyl alkoxy silane, vinyl alkoxy silane, employing acidic resins to make catalyzer, the preparation methyl phenyl vinyl polysiloxane; The patent No. CN10161917A such as the Liu Bai of the Chengdu Organical Chemical Co., Ltd., Chinese Academy of Sciences tinkling of pieces of jade by hexichol dichloro, diformazan, dimethyl vinyl, methyl hydrogen, dimethylamino hydrogen, phenylbenzene, methyl ethylene, make the vinyl benzene radical siloxane.The patent No. CN101323667A of Hangzhou Pedagogic University, employing water glass is main raw material, with phenyl alkoxyl group, vinyl alkoxy, methyl alkoxy hydrolysis, obtains the ethenylphenyl silicone resin of MQ structure; The patent No. CN1696179A of Harbin Institute of Technology, adopt alkoxychlorosilane, phenyl chlorosilane, vinyl chlorosilane, synthesize first the vinyl methyl phenyl silicone resin and give aggressiveness, add annular lamina nanometer type cage type polytope silsesquioxane again, graft reaction obtains silicone resin; The patent No. CN1810858A that the Zhou Yuan of Zhonglan Chenguang Chemical Inst builds etc., adopt the alkyl trialkoxy silanes such as phenyl triethoxysilane, the dialkyl dialkoxy silicanes such as aminomethyl phenyl diethoxy silane, phenylbenzene diethoxy silane, the toluene solution of the hydrolysis ethenylphenyl silicone resin such as tetraethoxy.These patents have mostly adopted the chlorine monomer, or water glass is main raw material, and the resin of working it out always has the bad problem of stability, and damage ratio is larger.
Summary of the invention
In order to solve above-mentioned technical problem, the purpose of this invention is to provide the preparation method of the silicone resin of the ethenylphenyl that encapsulates for LED, the method is easy and simple to handle, is conducive to the stable of product structure and quality.
In order to realize above-mentioned purpose, the present invention has adopted following technical scheme:
Be used for the preparation method of silicone resin of the ethenylphenyl of LED encapsulation, should be prepared by the method that may further comprise the steps:
1) adds water in the still; Solubilizing agent, the consumption of solvent are 20 ~ 60% of reaction system gross weight;
2) add closure agent, perhaps also add l, 2,3,4-tetrem thiazolinyl～1,2,3,4 one tetramethyl-ring tetrasiloxanes stir, and add acid catalyzer, described closure agent, its ethene base unit weight is 0 ~ 10%(wt) of resin quality;
3) behind above-mentioned mixed solution stirring at normal temperature 60s～1800s, under 0 ~ 60 ℃, be added dropwise to one or more the ethanolic soln in octadecyloxy phenyl TMOS, vinyl alkoxy silane, the tetraethoxy; Time for adding 30 ~ 300min; The consumption of described octadecyloxy phenyl TMOS, vinyl alkoxy silane, tetraethoxy is: its ethene base unit weight is 0 ~ 10%(wt) of resin quality, and its phenyl content is 0 ~ 80%(wt) of resin quality, and both can not be 0 simultaneously;
4) drip after, be under 10 ℃～100 ℃ conditions in temperature, cohydrolysis 30min～600min;
5) then, leave standstill 5 ~ 30h; Layering; Oil agent liquid with salt neutralization, extremely neutral with deionized water wash again, is left standstill 5 ~ 30h; Layering; Dry finish is to clear;
6) finish is used the condensation additive, at 20 ~ 100 ℃ of lower 1 ~ 6hr that process, again with finish vacuum tightness-0.0800 ~-0.0999Mpa, set aside low-boiling-point substance for 100 ~ 220 ℃, can obtain product ethenylphenyl silicone resin.
As preferably, above-mentioned step 1) solvent is selected one or more mixing in methyl alcohol, ethanol, Virahol, toluene and the dimethylbenzene.
As preferably, above-mentioned step 2) closure agent is hexamethyldisiloxane or l, 3～divinyl～1,1,3,3 one tetramethyl disiloxanes.
As preferably, above-mentioned step 2) an acidic catalyst is the hydrochloric acid of 15% ~ 36% weight percent concentration, the sulfuric acid of 98% weight percent concentration and one or more mixing in the phenylmethane sulfonic acid.
As preferably, above-mentioned step 3) octadecyloxy phenyl TMOS is one or more in aminomethyl phenyl dimethoxy silane, aminomethyl phenyl diethoxy silane, dimethoxydiphenylsilane, phenylbenzene diethoxy silane, phenyltrimethoxysila,e, phenyl triethoxysilane and the triphenyl methoxy silane; Vinyl alkoxy silane is one or more in methyl ethylene dimethoxy silane and the methyl ethylene diethoxy silane; The octadecyloxy phenyl TMOS is one or more in phenyltrimethoxysila,e, aminomethyl phenyl dimethoxy silane and the dimethoxydiphenylsilane; Vinyl alkoxy silane is the methyl ethylene diethoxy silane.
As preferably, the consumption of above-mentioned step 3) octadecyloxy phenyl TMOS, vinyl alkoxy silane, tetraethoxy is, its ethene base unit weight is 1%～7% of resin quality, and its phenyl content is 10%～60% of resin quality.
Be the ethanolic soln of tetraethoxy as preferred again, above-mentioned step 3) dropping.
As preferably, be in yellow soda ash, sodium bicarbonate, the liquefied ammonia aqueous solution and the hexamethyldisilazane one or more in the above-mentioned step 5) with salt.
As preferably, in the above-mentioned step 5) in the drying used siccative be in Calcium Chloride Powder Anhydrous, the anhydrous magnesium sulfate one or more.
As preferably, above-mentioned step 6) condensation additive is one or more in KOH, Tetramethylammonium hydroxide, hexamethyldisilazane, zinc acetate, zinc octoate, Zinc dibenzoate, cinnamic acid zinc and the aluminium isopropoxide.
The present invention is owing to having adopted above-mentioned technical scheme, by in water, solvent, add methyl closure agent, vinyl closure agent, vinyl ring body, an acidic catalyst, add octadecyloxy phenyl TMOS, vinyl alkoxy silane and aminomethyl phenyl organoalkoxysilane, phenylbenzene organoalkoxysilane, tetraethoxysilane etc. again, heating hydrolysis reacts; By standing demix, get oil reservoir, neutralization, washing, drying, condensation is processed, and removes low-boiling-point substance again, namely gets the ethenylphenyl silicone resin of water white transparency product.From Hangzhou Pedagogic University come the patent No. CN101475689B of state's bridge etc. different be that preparation method of the present invention does not adopt methyl alkoxy silane, so resin structure is fully different; Preparation technology, catalyzer are also fully different, more are conducive to the stable of product structure and quality.
The invention has the beneficial effects as follows: with the ethenylphenyl silicone resin of method preparation of the present invention, clear, refractive index is 1.46～1.55.Particularly at phenyl content 10wt%～60wt%, contents of ethylene 1wt%～7wt% is especially suitable for use as polymeric reinforcement agent in the LED packaged material.Present method raw material is cheap and easy to get, mild condition, and technique is simple, and is easy and simple to handle, is convenient to industrialization.
Embodiment
The below specifies enforcement of the present invention, but embodiment is not limiting the scope of the invention.
EXAMPLE l
In the 3000ml glass kettle, add entry 300m1, toluene 500ml, ethanol 300ml, MM20g, l, 3 one divinyl, one l, 1,3,3 one tetramethyl disiloxane 70g, concentrated hydrochloric acid (36.5wt%) 20g is at 40 ℃ of lower rapid stirrings, drip phenyltrimethoxysila,e 1000g, the ethanolic soln of aminomethyl phenyl dimethoxy silane 60g.Hydrolysis, then time 3h is warming up to 70 ℃ of backflow 5h, stopped reaction then, standing demix takes off a layer finish, with the sodium bicarbonate aqueous solution neutralization, again with deionized water wash to neutral, be dried to as clear as crystal with Calcium Chloride Powder Anhydrous.Add silazane 20 g, at 80 ℃ of reaction 3h, then heat up, pull out under high vacuum-0.099Mpa and be low to moderate 150 ℃, time 6h removes low-boiling-point substance, namely gets clear product ethenylphenyl silicone resin 807g.The products therefrom refractive power is 1.5145, viscosity 3300mPa.s, vinyl quality percentage composition 2.35%.
Embodiment 2
In the 3000ml glass kettle, add entry 300m1, toluene 500ml, ethanol 300ml, MM100g, l, 3 one divinyl, one l, 1,3,3 one tetramethyl disiloxane 150g, concentrated hydrochloric acid (36.5wt%) 20g is at 40 ℃ of lower rapid stirrings, drip phenyltrimethoxysila,e 900g, the ethanolic soln of tetraethoxy 20g.Hydrolysis, then time 3h is warming up to 70 ℃ of backflow 5h, then stopped reaction, standing demix takes off a layer finish, with the sodium bicarbonate aqueous solution neutralization, adds KOH30 g again, at 80 ℃ of reaction 3h, cooling, extremely neutral with deionized water wash again, be dried to as clear as crystal with Calcium Chloride Powder Anhydrous.Then heat up, pull out under high vacuum-0.099Mpa and be low to moderate 150 ℃, time 6h removes low-boiling-point substance, namely gets clear product ethenylphenyl silicone resin 827g.The products therefrom refractive power is 1.5142, viscosity 1953mPa.s, vinyl quality percentage composition 4.75%.
Embodiment 3
In the 3000ml glass kettle, add entry 300m1, toluene 500ml, ethanol 300ml, MM30g, l, 3 one divinyl, one l, 1,3,3 one tetramethyl disiloxane 170g, concentrated hydrochloric acid (36.5wt%) 22g is at 40 ℃ of lower rapid stirrings, drip phenyltrimethoxysila,e 800g, the ethanolic soln of aminomethyl phenyl dimethoxy silane 150g.Hydrolysis, then time 3h is warming up to 70 ℃ of backflow 5h, stopped reaction then, standing demix takes off a layer finish, with the sodium bicarbonate aqueous solution neutralization, again with deionized water wash to neutral, be dried to as clear as crystal with Calcium Chloride Powder Anhydrous.Add silazane 20 g, at 80 ℃ of reaction 3h, then heat up, pull out under high vacuum-0.099Mpa and be low to moderate 150 ℃, time 6h removes low-boiling-point substance, namely gets clear product ethenylphenyl silicone resin 840g.The products therefrom refractive power is 1.5356, viscosity 5358mPa.s, vinyl quality percentage composition 5.35%.
Embodiment 4
In the 3000ml glass kettle, add entry 300m1, toluene 380ml, ethanol 370ml, MM10g, l, 3 one divinyl, one l, 1,3,3 one tetramethyl disiloxane 170g, concentrated hydrochloric acid (36.5wt%) 22g is at 40 ℃ of lower rapid stirrings, drip phenyltrimethoxysila,e 800g, the ethanolic soln of aminomethyl phenyl dimethoxy silane 150g.Hydrolysis, then time 3h is warming up to 70 ℃ of backflow 5h, stopped reaction then, standing demix takes off a layer finish, with the sodium bicarbonate aqueous solution neutralization, again with deionized water wash to neutral, be dried to as clear as crystal with Calcium Chloride Powder Anhydrous.Add silazane 20 g, at 80 ℃ of reaction 3h, then heat up, pull out under high vacuum-0.099Mpa and be low to moderate 150 ℃, time 6h removes low-boiling-point substance, namely gets clear product ethenylphenyl silicone resin 832g.The products therefrom refractive power is 1.5406, viscosity 19358mPa.s, vinyl quality percentage composition 5.39%.
Embodiment 5
In the 20000ml glass kettle, add entry 1200m1, toluene 1920ml, ethanol 1480ml, MM30g, l, 3 one divinyl, one l, 1,3,3 one tetramethyl disiloxane 700g, concentrated hydrochloric acid (36.5wt%) 100g, at 40 ℃ of lower rapid stirrings, drip phenyltrimethoxysila,e 3000g, aminomethyl phenyl dimethoxy silane 1000g, the ethanolic soln of tetraethoxy 200g.Hydrolysis, then time 3h is warming up to 70 ℃ of backflow 5h, stopped reaction then, standing demix takes off a layer finish, with the sodium bicarbonate aqueous solution neutralization, again with deionized water wash to neutral, be dried to as clear as crystal with Calcium Chloride Powder Anhydrous.Add silazane 50 g, at 80 ℃ of reaction 3h, then heat up, pull out under high vacuum-0.099Mpa and be low to moderate 150 ℃, time 6h removes low-boiling-point substance, namely gets clear product ethenylphenyl silicone resin 3532g.The products therefrom refractive power is 1.5435, viscosity 18730mPa.s, vinyl quality percentage composition 5.31%.
Embodiment 6
In the 3000ml glass kettle, add entry 300m1, toluene 500ml, ethanol 400ml, MM60g, l, 3 one divinyl, one l, 1,3,3 one tetramethyl disiloxane 160g, concentrated hydrochloric acid (36.5wt%) 22g is at 40 ℃ of lower rapid stirrings, drip phenyltrimethoxysila,e 900g, the ethanolic soln of aminomethyl phenyl dimethoxy silane 20g.Hydrolysis, then time 3h is warming up to 70 ℃ of backflow 5h, then stopped reaction, standing demix takes off a layer finish, with the sodium bicarbonate aqueous solution neutralization, adds KOH30 g again, at 80 ℃ of reaction 3h, cooling, extremely neutral with deionized water wash again, be dried to as clear as crystal with Calcium Chloride Powder Anhydrous.Then heat up, pull out under high vacuum-0.099Mpa and be low to moderate 150 ℃, time 6h removes low-boiling-point substance, namely gets clear product ethenylphenyl silicone resin 812g.The products therefrom refractive power is 1.5231, viscosity 5920mPa.s, vinyl quality percentage composition 5.17%.
Embodiment 7
In the 50000ml glass kettle, add entry 3900m1, toluene 6500ml, ethanol 4800ml, MM350g, l, 3 one divinyl, one l, 1,3,3 one tetramethyl disiloxane 2280g, concentrated hydrochloric acid (36.5wt%) 300g is at 40 ℃ of lower rapid stirrings, drip phenyltrimethoxysila,e 12700g, the ethanolic soln of aminomethyl phenyl dimethoxy silane 220g.Hydrolysis, then time 3h is warming up to 70 ℃ of backflow 5h, stopped reaction then, standing demix takes off a layer finish, with the sodium bicarbonate aqueous solution neutralization, again with deionized water wash to neutral, be dried to as clear as crystal with Calcium Chloride Powder Anhydrous.Add silazane 220 g, at 80 ℃ of reaction 3h, then heat up, pull out under high vacuum-0.099Mpa and be low to moderate 150 ℃, time 6h removes low-boiling-point substance, namely gets clear product ethenylphenyl silicone resin 10551g.The products therefrom refractive power is 1.5300, viscosity 20820mPa.s, vinyl quality percentage composition 5.80%.
Embodiment 8
In the 50000ml glass kettle, add entry 3900m1, toluene 6500ml, ethanol 5200ml, MM1600g, l, 3 one divinyl, one l, 1,3,3 one tetramethyl disiloxane 970g, concentrated hydrochloric acid (36.5wt%) 300g is at 40 ℃ of lower rapid stirrings, drip phenyltrimethoxysila,e 12300g, the ethanolic soln of aminomethyl phenyl dimethoxy silane 220g.Hydrolysis, then time 3h is warming up to 70 ℃ of backflow 5h, stopped reaction then, standing demix takes off a layer finish, with the sodium bicarbonate aqueous solution neutralization, again with deionized water wash to neutral, be dried to as clear as crystal with Calcium Chloride Powder Anhydrous.Add silazane 220 g, at 80 ℃ of reaction 3h, then heat up, pull out under high vacuum-0.099Mpa and be low to moderate 150 ℃, time 6h removes low-boiling-point substance, namely gets clear product ethenylphenyl silicone resin 10283g.The products therefrom refractive power is 1.5233, viscosity 15220mPa.s, vinyl quality percentage composition 2.53%.
At last, it is also to be noted that, what more than enumerate only is specific embodiments of the invention.Obviously, the invention is not restricted to
State embodiment, can also many operative combination.Those of ordinary skill in the art can directly derive from content disclosed by the invention
Or all scenario of associating, all should think protection scope of the present invention.
Claims (10)
1. be used for the preparation method of silicone resin of the ethenylphenyl of LED encapsulation, it is characterized in that this is prepared by the method that may further comprise the steps:
1) adds water in the still; Solubilizing agent, the consumption of solvent are 20 ~ 60% of reaction system gross weight;
2) add closure agent, perhaps also add l, 2,3,4-tetrem thiazolinyl～1,2,3,4 one tetramethyl-ring tetrasiloxanes stir, and add acid catalyzer, described closure agent, its ethene base unit weight is 0 ~ 10%(wt) of resin quality;
3) behind above-mentioned mixed solution stirring at normal temperature 60s～1800s, under 0 ~ 60 ℃, be added dropwise to one or more the ethanolic soln in octadecyloxy phenyl TMOS, vinyl alkoxy silane, the tetraethoxy; Time for adding 30 ~ 300min; The consumption of described octadecyloxy phenyl TMOS, vinyl alkoxy silane, tetraethoxy is: its ethene base unit weight is 0 ~ 10%(wt) of resin quality, and its phenyl content is 0 ~ 80%(wt) of resin quality, and both can not be 0 simultaneously;
4) drip after, be under 10 ℃～100 ℃ conditions in temperature, cohydrolysis 30min～600min;
5) then, leave standstill 5 ~ 30h; Layering; Oil agent liquid with salt neutralization, extremely neutral with deionized water wash again, is left standstill 5 ~ 30h; Layering; Dry finish is to clear;
6) finish is used the condensation additive, at 20 ~ 100 ℃ of lower 1 ~ 6hr that process, again with finish vacuum tightness-0.0800 ~-0.0999Mpa, set aside low-boiling-point substance for 100 ~ 220 ℃, can obtain product ethenylphenyl silicone resin.
2. the preparation method of the silicone resin of the ethenylphenyl for LED encapsulation according to claim 1, it is characterized in that: the step 1) solvent is selected one or more mixing in methyl alcohol, ethanol, Virahol, toluene and the dimethylbenzene.
3. the preparation method of the silicone resin of the ethenylphenyl for LED encapsulation according to claim 1 is characterized in that: step 2) closure agent is hexamethyldisiloxane or l, 3～divinyl～1,1,3,3 one tetramethyl disiloxanes.
4. the preparation method of the silicone resin of the ethenylphenyl for LED encapsulation according to claim 1 is characterized in that: step 2) an acidic catalyst is the hydrochloric acid of 15% ~ 36% weight percent concentration, the sulfuric acid of 98% weight percent concentration and one or more mixing in the phenylmethane sulfonic acid.
5. the preparation method of the silicone resin of the ethenylphenyl for LED encapsulation according to claim 1, it is characterized in that: step 3) octadecyloxy phenyl TMOS is one or more in aminomethyl phenyl dimethoxy silane, aminomethyl phenyl diethoxy silane, dimethoxydiphenylsilane, phenylbenzene diethoxy silane, phenyltrimethoxysila,e, phenyl triethoxysilane and the triphenyl methoxy silane; Vinyl alkoxy silane is one or more in methyl ethylene dimethoxy silane and the methyl ethylene diethoxy silane; The octadecyloxy phenyl TMOS is one or more in phenyltrimethoxysila,e, aminomethyl phenyl dimethoxy silane and the dimethoxydiphenylsilane; Vinyl alkoxy silane is the methyl ethylene diethoxy silane.
6. the preparation method of silicone resin who is used for according to claim 1 or 5 the ethenylphenyl of LED encapsulation, it is characterized in that: the consumption of step 3) octadecyloxy phenyl TMOS, vinyl alkoxy silane, tetraethoxy is, its ethene base unit weight is 1%～7% of resin quality, and its phenyl content is 10%～60% of resin quality.
7. the preparation method of the silicone resin of the ethenylphenyl for LED encapsulation according to claim 6, it is characterized in that: it is the ethanolic soln of tetraethoxy that step 3) drips.
8. the preparation method of the silicone resin of the ethenylphenyl for LED encapsulation according to claim 1 is characterized in that: in the step 5) with salt be in yellow soda ash, sodium bicarbonate, the liquefied ammonia aqueous solution and the hexamethyldisilazane one or more.
9. the preparation method of the silicone resin of the ethenylphenyl for LED encapsulation according to claim 1 is characterized in that: in the step 5) in the drying used siccative be in Calcium Chloride Powder Anhydrous, the anhydrous magnesium sulfate one or more.
10. the preparation method of the silicone resin of the ethenylphenyl for LED encapsulation according to claim 1, it is characterized in that: step 6) condensation additive is one or more in KOH, Tetramethylammonium hydroxide, hexamethyldisilazane, zinc acetate, zinc octoate, Zinc dibenzoate, cinnamic acid zinc and the aluminium isopropoxide.
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| CN103360603A (en) * | 2013-06-21 | 2013-10-23 | 深圳市森日有机硅材料有限公司 | Phenyl vinyl silicone resin for packaging LED (light-emitting diode) and preparation method thereof |
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